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Synthesis process with amide zymoid method for pressure reduction azeotropy continuous water elimination

A technology of enzymatic synthesis and amides, applied in the direction of fermentation, can solve the problems of aging service life, high investment cost and inability to apply

Inactive Publication Date: 2009-05-13
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Molecular sieve adsorption method is convenient and easy to implement, with obvious effect, and is often used in laboratory research. However, since the regeneration of molecular sieve after adsorption saturation requires special equipment and technology, the investment cost is high, so it cannot be applied in large-scale industrial production.
Membrane separation and water absorption method is theoretically feasible, but it is still difficult to realize due to problems such as membrane ducer, aging and service life.
Use tert-amyl alcohol, tert-butanol, etc., which can be compatible with enzymes to ensure the catalytic activity of enzymes, and can form an azeotropic mixture with the generated water as the reaction medium and water agent, and use negative pressure azeotropic distillation It is a good choice to take the water away by means of water, but unfortunately, the formed azeotropic mixture does not separate after condensation, so the continuous separation of water and the continuous recycling of solvent cannot be realized. The distilled water-containing solvent must be After special drying treatment, it can be reused
Drying costs of aqueous solvents greatly limit the application of this technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0013] 90g (1mol) of methoxyacetic acid, 121g (1mol) of racemic phenethylamine and 5g of Novozym 435 were added to 500ml of anhydrous tert-amyl alcohol to form a mixture, then at 55°C, under constant stirring, the reaction 8hr. Then add 100ml of cyclohexane, turn on the vacuum pump, and reduce the pressure of the reaction system to 0.001-0.005MPa, so that the azeotropic mixed steam is evaporated, and the steamed mixed steam is condensed and separated into layers to form a cyclohexane phase and an aqueous phase , the cyclohexane phase automatically returns to the reaction system for recycling. The reaction system continued to maintain the reaction while distilling off, condensing, and refluxing in this state until the volume of the water phase in the water-splitting condenser no longer increased, and continued to maintain the reaction for 4hr. After the reaction is finished, the reaction mixture is filtered to separate the solid enzyme, and then the solvent and the water-carry...

example 2

[0015] 22g of lauric acid, 14g of lysine and 1g of Aspergillus niger-derived lipase were added to 100ml of anhydrous tert-butanol to form a mixture, and then reacted at 36°C for 12hr under constant stirring. Then add 10ml of hexane, turn on the vacuum pump, reduce the pressure of the reaction system to 0.001-0.005MPa, so that the azeotropic mixed steam is evaporated, and the steamed mixed steam is condensed and separated into layers to form a hexane phase and an aqueous phase. The hexane phase automatically returns to the reaction system for recycling. The reaction system continued to maintain the reaction while evaporating, condensing, and refluxing in this state until all lysine solids disappeared in the reaction system, and the volume of the water phase in the water-splitting condenser no longer increased, and continued to maintain the reaction for 4hr. After the reaction is finished, the reaction mixture is filtered to separate the solid enzyme, and then the solvent and th...

example 3

[0018] 135g of L-aspartic acid, 117g of ethyl D-alanine and 1g of neutral protease were added to 100ml of anhydrous tert-butanol to form a mixture, and then reacted at 36°C for 12hr under constant stirring. Then add 10ml of pentane, turn on the vacuum pump, reduce the pressure of the reaction system to 0.01-0.005MPa, so that the azeotropic mixed steam is evaporated, and the steamed mixed steam is condensed and separated to form a pentane phase and an aqueous phase. The alkane phase automatically returns to the reaction system for recycling. The reaction system continued to maintain the reaction while evaporating, condensing, and refluxing in this state until all the shikimic acid solids disappeared in the reaction system, and the volume of the water phase in the water-splitting condenser did not increase any more, and continued to maintain the reaction for 4 hours. After the reaction is finished, the reaction mixture is filtered to separate the solid enzyme, and then the solve...

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Abstract

The invention belongs to the field of nonaqueous phase enzymatic organic synthesis application biotechnology, and in particular relates to a process of amide-type enzymatic synthesis by decompressed azeotropic continuous dehydration. The process is generally suitable for synthesis of various amido bonds catalyzed by biocatalyst (such as neutral protease). The invention provides a generally practicable novel process for amide-type enzymatic synthesis; and under the premise of not affecting catalytic activity of the biocatalyst, through decompressed azeotropic continuous dehydration, reaction balance moves to the synthetic direction of amide, so as to improve conversion rate of enzymatic organic synthesis greatly, ensure that the reaction tends to finish, solve the continuous water-removing problem in the nonaqueous phase enzymatic organic synthesis thoroughly, improve purity and yield of products, reduce production cost, and have wide application prospect in the fields such as medicine, food, material, fine chemical industry and the like.

Description

technical field [0001] The invention belongs to the field of applied biotechnology of non-aqueous phase enzymatic organic synthesis, in particular to an amide enzymatic synthesis process of decompression azeotropic continuous water removal. Background technique [0002] Regarding the synthesis of amides, there are two methods of chemical synthesis and biocatalytic synthesis. The chemical synthesis process is very mature, and is still widely used in the industrial production of amides organic compounds. But there are some fatal flaws in the chemical synthesis process. This process often requires the use of strong liquid acids such as concentrated sulfuric acid or p-methoxybenzenesulfonic acid as a catalyst, and the reaction temperature is very high, usually accompanied by unavoidable side reactions, which have a great impact on the conversion rate of raw materials and the yield of products. Large, the separation and purification process is complicated, and it also has extre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P13/02
Inventor 汤鲁宏王择戴阿娟邓超陈伟刘平静
Owner JIANGNAN UNIV